Process of purifying ergosterol



Patented Sept, 9, 1930 .UNITED ATESPA E OFFICE EVERETT BILLS, or EVANSVIIZICE, INDIANA, ASSIGNOR 'ro MEAD Jonson a COMPANY, or EVANSVILLE, INDIANA, A CORPORATION or mnmiu.

PROCESS OF PURIEYING ERGOSTEROL This invention relates to the processes of purifying ergosterol.

This application is a division of my copending application, Serial No. 268,7 91, filed April 9, 1928, covering my invention in processes of preparing ergosterol.

The process of purifying ergosterol which is set forth, described, and claimed herein may be used to purify crude ergosterol prepared by the method disclosed-in my said copending application or may be used to purify ergosterol made by methods other than that referred to.

The main object of the present invention is to improve the art of refining ergosterol, to

w the end that substantially pure ergosterol,

free from other lipoids and sterols, may be produced.

. Another object is to device a method where-' by the desired result maybe attained with a mini-mum'ofexpense and manipulation of the crude ergostero foun To appreciate my inventionit should be understood that ergosterol is a sterol that occurs in minute amounts in a wide variety of ve etable and animal tissues. It is usually in association with other lipoids, especially with other sterols, and when prepared from the customary raw material, for example, from the fatty matter of fungi, it is almost alwa s contaminated with said sterols and lipoids. Such contaminated ergosterol is extremely diflicult to purify by crystallization from ordinar solvents. The reason for this appears to ethat the contaminants tend to crystallize out with the ergosterol when the usual sterol solvents, such ,as alcohol, acetone, ether, benzene, etc., are

A impurities, but the ergosterol so obtained, al-

though it maylook colorless and cr' stalline,

nevertheless remains impure, as may e shown by a determination of its specific rotation. 4 My process ofpurifying er osterol consists in employing a mixture 0 acetone and I ethyl other as a solvent for the crystallizationiof the ergosterol. By a systematic study of many individual solvents and solvent m x- No Drawing. Original application filed April 9, 1928, Serial Ira-265,791. Divided and this application filed April 15, 1929,

Serial No. 355,440.

tures I have discovered that acetone-ether mixtures permit an exceptionally rapid growth of ergosterol crystals, the crystals being not only large and perfect, but distinctly less contaminated than when other solvents are used.

In practicing my invention I dissolve ergosterol in a mixture of acetone and ether at or near the boiling point,- then allow'the solution to cool, and then collect the crystalsand work up the motheriliquor in the usual manner familiar to chemists. Preferably the mixture is composed of three volumes of acetone and one volume ofether, but variations that its specific rotation in chloroform will be -1209 for sodium light, and a few repetitions of the treatment produce ergosterol of extreme purity, the specific rotation being -132?,; As a specific example, in order to illustrate my invention, the following may be cited :.--10() grams of crude ergosterol (specific rotation for sodium light being -111 in chloroform) were dissolved in 5 liters of a boiling mixture consisting of three volumes of acetone and one volume of ethyl ether. ,The solution was cooled to 0- C., and the crystals obtained were then recrystallized three times more in the same manner. The final product exhibited a specific rotation of -131.", and was therefore of excellent purity The final yield, excluding second crops, amounted to 60 grams. I claim as myinventione- 1. An improvement in the process of purifying ergosterol which consists in crystalwhich consists in crystallizing the ergosterol from a mixture of acetone and ether in the proportion of three parts by volume of acetone and one part by volume of ether, collectingthe cr stals, and subjecting the same to recrystallization.

5. An improvement in the process of purifying ergosterol which consists in crystallizing ergosterol from a mixture of acetone and ether and collecting the crystals romptly after they have been formed ami before 6. An improvement in the process of purifying ergosterol 4 which conslsts in using a mixture of acetone, three parts by volume, and ether, one part by volume, as a solvent for crystallization of the ergosterol, and collecting the crystals romptly after they have been formed and be ore precipitation of other sterols occurs.

7. An improvementin the process of puri- "precipitation of other sterols occurs.

fying ergosterol which consists in crystallizing ergosterol from a mixture of acetone and ether, collecting the crystals promptly after they have been formed and before precipitation of other sterols occurs and subecting the crystals to re-crystallization.

8. An improvement in the process of puri- 'fying ergosterol which consists in uslng a mixture of acetone, three parts by volume, and ether, one part by volume, as a solvent for crystallization of the ergosterol, collecting the crystals (promptly after they have been formed' an be ore precipitation of other sterols occurs and sub ecting the crystals to re-crystallization.

S}. An improvement in the process of puritying ergosterol which consists in crystallizng ergosterol from a mixture of acetone and ether as a solvent, using approximately 50 cc. of solvent to one gram of ergosterol.

10. An improvement in the process of purifymg ergosterol which consists in using a mixture'of acetone, three parts by volume, and ether, one for crystallization of the ergosterol, using approximately 50 cc. of the gram of ergosterol."

11. An improvement in the process of purifylng ergosterol which consists in crystallizing ergosterol from a mixture of acetone and ether as a solvent, using approximately art by volume, as a solvent solvent to oneas my invention, I afiix my signature, this 8th day of April, 1929.

CHARLES EVERETT BILLS. 

